TY - JOUR A1 - Matoga, D. A1 - Roztocki, K. A1 - Wilke, Manuel A1 - Emmerling, Franziska A1 - Oszajca, M. A1 - Fitta, M. A1 - Bałanda, M. T1 - Crystalline bilayers unzipped and rezipped: solid-state reaction cycle of a metal–organic framework with triple rearrangement of intralayer bonds N2 - We present a series of remarkable structural transformations for a family of layered metal–organic frameworks (MOFs) in a three-step solid-state reaction cycle. The cycle represents new dynamic behavior of 2D coordination polymers and involves the sequence of reactions: {[Mn2(ina)4(H2O)2]·2EtOH}n (JUK-1) → {(NH4)2[Mn(ina)2(NCS)2]}n·xH2O (JUK-2) → {[Mn2(ina)2(Hina)2(NCS)2]}n (JUK-3) → JUK-1 (Hina = isonicotinic acid), each accompanied by rearrangement of intralayer coordination bonds and each induced by a different external stimulus. In situ investigation of the first step of the cycle by combined synchrotron X-ray diffraction and Raman spectroscopy reveals direct mechanochemical unzipping of JUK-1 bilayers to respective JUK-2 layers with reaction rates dependent on the milling conditions. In contrast, the reverse zipping of JUK-2 layers involves two steps and proceeds through a new MOF (JUK-3) whose structure was elucidated by powder X-ray diffraction. Magnetic measurements confirm conversions of manganese nodes in the reaction cycle. The findings indicate the possibility of developing coordination-based assemblies with large structural responses for use in smart stimuli-responsive systems and sensor technologies. KW - Mechanochemistry KW - In situ KW - XRD KW - MOF PY - 2017 UR - http://pubs.rsc.org/is/content/articlehtml/2017/ce/c7ce00655a DO - https://doi.org/10.1039/C7CE00655A VL - 19 SP - 2987 EP - 2995 AN - OPUS4-41517 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wilke, Manuel A1 - Kabelitz, Anke A1 - Zimathies, Annett A1 - Rademann, K. A1 - Emmerling, Franziska T1 - Crystal structure and in situ investigation of a mechanochemical synthesized 3D zinc N-(phosphonomethyl)glycinate N2 - The mechanochemical synthesis of the zinc N-(phosphonomethyl)glycinate Zn(O₃PCH₂NH₂CH₂CO₂) H₂O is presented. The structure was solved from powder X-ray diffraction (PXRD) data. In the three-dimensional pillared structure, the Zn atoms are coordinated tetrahedrally. In situ investigations of the reaction process with synchrotron PXRD and Raman spectroscopy reveal a two-step process including the formation of an intermediate. KW - Mechanochemistry KW - Metal phosphonate KW - In situ PY - 2017 DO - https://doi.org/10.1007/s10853-017-1121-7 SN - 0022-2461 SN - 1573-4803 VL - 52 IS - 20 SP - 12013 EP - 12020 PB - Springer CY - New York AN - OPUS4-41490 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kulla, Hannes A1 - Fischer, Franziska A1 - Benemann, Sigrid A1 - Rademann, K. A1 - Emmerling, Franziska T1 - The effect of the ball to reactant ratio on mechanochemical reaction times studied by in situ PXRD N2 - The effect of the reactant powder mass on reaction times for the mechanochemical formation of a soft matter model system was studied by in situ PXRD. The syntheses were performed at a constant ball mass in a shaker mill with and without glassy SiO2 as an inert additive. Reaction times decreased with the increase of the ball to reactant ratio (BRR). The kinetic influence of the SiO2 powder was excluded. The decrease in the reaction time with decreasing mass of reactants was related to the rise in the stress energy transferred to the powder by a higher ball impact. The BRR had no effect on the induction time. But the product conversion was accelerated by raising the BRR. While a certain temperature is needed for the activation of reactants in the induction phase, the conversion of soft matter reactants is rather controlled by impact than temperature. KW - XRD KW - Mechanochemistry PY - 2017 UR - http://pubs.rsc.org/en/content/articlehtml/2017/ce/c7ce00502d DO - https://doi.org/10.1039/c7ce00502d VL - 19 IS - 28 SP - 3902 EP - 3907 AN - OPUS4-41197 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lohrer, Christian A1 - Fink, Heidrun A1 - Kurth, Lutz T1 - Quality systems for fireworks - auditing experiences by the notified body BAM N2 - The coming into force of the European Directive 2007/23/EC of the European Parliament and of the Council of 23 May 2007 on the placing on the market of pyrotechnic articles changed the Situation regarding fireworks productions and tests in Europe significantly. According to the provisions of this Directive, the manufacturers/importers have to assure that fireworks articles are type tested by a Notified Body (or on behalf of a Notified Body) under this Directive before being placed on the European market and fulfill the essential safety requirements as per Annex I of the Directive 2007/23/EC. In addition, it is mandatory that the articles produced after the initial type test will be in conformity to the introduced type. The best sustainable way to assure this is the application of effective quality Systems (QS). Germany has a comparatively long tradition regarding auditing of such QS. Since 1978 it is mandatory for manufacturers/importers to set up adequate QS. The respective QS were extensively audited since the beginning of the 1990s in various countries to cover imported fireworks that were tested in a foreign country where the production took place. Within this long term auditing process in Germany, the QS strategies and contents changed in time due to new regulations and Standards, as well as gaining experiences (“lessons learned”). Recent audits carried out by BAM showed significant nonconformities in the QS of several Companies. Moreover, numerous small importers in Europe might be overwhelmed by the new regulations, leading to situations where products are placed on the European market, which were not sufficiently tested. This paper aims at giving an overview of the various advantages and weak points of all possible conformity assessment procedures regarding QS as set out in the Annex II of the Directive 2007/23/EC for fireworks, taking into account comprehensive experiences in this field by the Notified Body, BAM. T2 - 13th International symposium on fireworks CY - Valletta, Malta DA - 23.04.2012 KW - 2007/23/EC KW - QS modules KW - Product safety PY - 2012 SN - 978-0-9867279-3-1 SP - 159 EP - 172 AN - OPUS4-25796 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Löhnert, Andrea A1 - Rabe, Frederik A1 - Knaust, Christian A1 - Krause, U. T1 - Numerical and experimental investigation of fire smoke toxicity N2 - To predict the toxic hazards of fire smoke the concept of the Fractional Effective Dose (FED) is used (ISO13571 2012, ISO13344 2004). The Fractional Effective Doses of the main components from the fire smoke (CO, CO2, HCN etc.) are formed for every minute of the exposure interval and then summed up. If the sum of all doses over the exposure time reaches the value 1, incapacitation or death occurs (ISO13571 2012). T2 - International congress ' Fire computer modeling' CY - Cantabria, Spain DA - 18.10.2012 PY - 2012 SN - 978-84-86116-69-9 SP - 171 EP - 188 AN - OPUS4-27893 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lohrer, Christian A1 - Kampa, Andreas A1 - Fink, Heidrun A1 - Kurth, Lutz A1 - Alef, G. T1 - Burst height measurements of spherical shells for different calibers and mortar lengths N2 - The current European draft Standard series FprEN 16261:2012 for display fireworks gives requirements on mortar lengths for different calibers to be used in the respective type and batch tests of spherical Shells. For each nominal shell caliber, a minimum and maximum permitted mortar length is defined. The mortar lengths deviations increase by increasing nominal calibers and the possible influence on the bürst height can only roughly be estimated. The aim of this work was to specify this influence of the mortar length on the bürst height of spherical Shells with regard to the permitted tolerances on performance parameters in type and batch tests as given in FprEN 16261-2:2012. Moreover, commonly used height measuring techniques were parallel taken to determine the bürst heights and were compared to each other in order to find an optimal test method for such measurements concerning accuracy, handling, application and costs. The following spherical Shells were part of this study: • Caliber 65 mm red peony, • Caliber 100 mm red peony, • Caliber 150 mm red peony, and • Caliber 200 yellow to blue - white flashing. For each caliber type, 15 single items were fired: 7 from the mortar offering the required minimum length and 8 from the mortar close to the required maximum length according to FprEN 16261:2012. T2 - 13th International symposium on fireworks CY - Valletta, Malta DA - 23.04.2012 KW - Altitude measurement techniques KW - Measurement uncertainties KW - Standardisation PY - 2012 SN - 978-0-9867279-3-1 SP - 145 EP - 158 AN - OPUS4-25795 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lueck, S. A1 - Kupsch, Andreas A1 - Lange, Axel A1 - Hentschel, Manfred P. A1 - Schmidt, V. T1 - Statistical comparison of various reconstruction algorithms with respect to missing wedge artifacts in computed tomography N2 - The presence of elongation, streak and blurring artifacts in tomograms recorded under a missing wedge of rotation angles presents a major challenge for the quantitative analysis of tomographic image data. We show that the missing wedge artifacts of standard reconstruction algorithms may be reduced by the innovative reconstruction technique DIRECTT. For the comparison of missing wedge artifacts we apply techniques from spatial statistics, which have been specifically designed to investigate the shape of phase boundaries in tomograms. KW - X-ray tomography KW - Scanning transmission electron microscopy (STEM) KW - Structural PY - 2012 DO - https://doi.org/10.1557/opl.2012.209 SN - 0272-9172 VL - 1421 SP - 1 EP - 6 PB - North-Holland Publ. Co. CY - New York, NY AN - OPUS4-25468 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bernal, S. A. A1 - Angst, U. M. A1 - Provis, J. L. A1 - Thiel, C. A1 - Gluth, Gregor A1 - Villagran-Zaccardi, Y. A1 - De Belie, N. T1 - Recommendation of RILEM TC 281-CCC: RILEM CPC-18R1—guideline for measuring the carbonation depth of hardened concrete using a pH indicator solution N2 - This recommendation provides a procedure for determining the carbonation depth on the surface of concrete by applying a pH indicator. This includes definitions of carbonation, carbonation depth and carbonation front, as well as descriptions of the different pH indicator solutions that can be used. Recommendations for testing laboratory-prepared specimens and those obtained from concrete structures are also given. This involves guidelines for sample preparation and/or extraction, CO2 exposure duration, carbonation depth determination and reporting of results. A section on data interpretation is also provided, as carbonation results are used for determining durability of concrete, as well as a criterion for materials selection or for carbon uptake calculations. The new Recommendation CPC-18R1 is intended to supersede the former RILEM recommendation CPC-18, particularly when prescribed as the preferred method for evaluating and reporting carbonation depths. KW - Carbonation KW - Concrete KW - pH indicator KW - Phenolphthalein KW - Testing PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-656191 DO - https://doi.org/10.1617/s11527-026-02966-0 SN - 1359-5997 SN - 1871-6873 VL - 59 IS - 3 SP - 1 EP - 11 PB - Springer Nature AN - OPUS4-65619 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scholl, Juliane A1 - Scharpmann, Philippa A1 - Bagheri, Abbas A1 - Lisec, Jan A1 - Meiers, Emelie A1 - Jaeger, Carsten A1 - Leonhardt, Robert A1 - Haase, Hajo A1 - Koch, Matthias T1 - Beyond the lab: Real-world composition of commercial Li-ion battery electrolytes N2 - This study presents a systematic, characterization of electrolytes from commercial lithium-ion batteries (LIB), encompassing 90 batteries from leading global manufacturers across diverse formats and application sectors. An integrated, complementary mass spectrometric workflow combining LC–MS/MS, GC–MS, and high-resolution MS was employed. To ensure robust structural annotation, molecular identifications were assigned confidence levels following Schymanski et al. (2014). Across all formats, PF6− was confirmed as the dominant Li+ counterion, frequently coexisting with BF4−, PO2F2−, and bis(fluorosulfonyl)imide (FSI−), forming binary and ternary salt systems optimized for both conductivity and safety. Solvent systems revealed the widespread use of propylene carbonate (PC) combined with diverse carbonate mixtures, demonstrating trends in performance optimization specific to cell format. A variety of additives were identified, reflecting a clear shift towards multifunctional, synergistic additive packages and the gradual replacement of fluorinated species with environmentally safer alternatives. Cycling studies demonstrated that electrolyte degradation mechanisms are strongly influenced by electrode composition and additive chemistry, with oxidative degradation pathways dominating. Together, these findings provide rare empirical insight into the evolving formulation strategies of electrolytes in commercial LIB, still employing classic carbonates and LiPF6, but highlighting a trend toward safer, more robust, and sustainable electrolyte architectures by using synergistic multifunctional systems. KW - Mass Spectrometry KW - Lithium-ion batteries KW - Electrolyte degradation PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-656254 DO - https://doi.org/10.1016/j.jpowsour.2026.239739 SN - 0378-7753 VL - 673 SP - 1 EP - 13 PB - Elsevier B.V. AN - OPUS4-65625 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lange, Axel A1 - Hentschel, Manfred P. A1 - Kupsch, Andreas A1 - Müller, Bernd R. T1 - Numerical correction of X-ray detector backlighting N2 - A novel approach to strongly suppress artifacts in radiography and computed tomography caused by the effect of diffuse background signals ('backlighting') of 2D X-ray detectors is suggested. Depending on the detector geometry the mechanism may be different, either based on the optical scattering by the fluorescent screen materials into optical detection devices or Compton or X-ray fluorescence scattering by the detector components. Consequently, these erroneous intensity portions result in locally different violations of Lambert–Beer's law in single projections (radiographs). When used as input data for computed tomography these violations are directly observed via modulation of the projected mass as a function of the rotation phase and the sample’s aspect ratio (dynamics). The magnitude of the diffuse background signal depends on the detector area covered by the projected sample. They are more pronounced the smaller the shadowed area and the stronger the total attenuation. This implies that the reconstruction suffers from additional anisotropic artifacts caused by elongated sample structures. This issue is studied simply by absorption of flat plates in a conventional laboratory radiography set-up and at a synchrotron radiation facility. In the latter case beam hardening artifacts can be excluded due to the monochromatic radiation. The proposed correction procedure requires simple integral intensity offsets as a constant (non-local) light scattering mechanism is assumed. KW - Detector backlighting KW - X-ray detector scattering KW - Fluorescent screen KW - Diffuse background KW - Computed tomography PY - 2012 DO - https://doi.org/10.3139/146.110659 SN - 1862-5282 VL - 103 IS - 2 SP - 174 EP - 178 PB - Carl Hanser CY - München AN - OPUS4-25553 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Krebber, Katerina A1 - Lenke, Philipp A1 - Liehr, Sascha A1 - Nöther, N. A1 - Wendt, Mario A1 - Wosniok, Aleksander A1 - Daum, Werner T1 - Structural health monitoring by distributed fiber optic sensors embedded into technical textiles N2 - Technical textiles with embedded distributed fiber optic sensors have been developed for the purposes of structural health monitoring in geotechnical and civil engineering. The distributed fiber optic sensors are based on Brillouin scattering in silica optical fibers and OTDR in polymer optical fibers. Such 'smart' technical textiles are used for reinforcement of geotechnical and masonry structures. The embedded fiber optic sensors provide online information about the condition of the structure and about the occurrence and location of any damage or degradation. N2 - Technische Textilien mit integrierten faseroptischen Sensoren eröffnen neue Möglichkeiten der Zustandsüberwachung (structural health monitoring) in Geotechnik und Ingenieurbau. Die verteilt messenden Sensoren basieren auf der Brillouin-Streuung in Glasfasern und auf der OTDR in polymeroptischen Fasern. Derartige 'intelligente' technische Textilien werden in erster Line zur Verstärkung von geotechnischen Bauwerken und von Gebäuden genutzt. Die integrierten Sensoren liefern eine zeitnahe Information über den bestimmungsgemäßen Zustand des Bauwerks sowie über die Entstehung und den Ort von lokalen Bauwerksschäden. KW - Fiber optic sensor KW - Distributed sensor KW - Brillouin scattering KW - Polymer optical fiber KW - Strain sensor KW - Smart geotextiles KW - Faseroptischer Sensor KW - Verteilter Sensor KW - Brillouin-Streuung KW - Polymeroptische Faser KW - Dehnungssensor KW - Intelligentes Geotextil PY - 2012 DO - https://doi.org/10.1524/teme.2012.0238 SN - 0340-837X SN - 0178-2312 SN - 0171-8096 VL - 79 IS - 7-8 SP - 337 EP - 347 PB - Oldenbourg CY - München AN - OPUS4-26387 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -